Process of obtaining nicotin.



' iatented m 16, 1901s".

ALFRED TKOEILLIKER, or IBEUEL, GERMANY.

PROCESS OF OBTAINlNG NlCOTlH- SPECIFICATION forming part of Letters Patent No. 190,138, May

' Application fina November 30,1903. Serial in. 183,215.

'To a. whom it may coiwcrn:

Be it-known that I. ALFRED KosLLIKER,

v manufacturing chemist, of 4 .Nordstrasse,

Beu elon-the-Rhine, in the German Empire,

have invented a. new and useful Method of Producing Nicotin and Its Salts; and I declare the following to be a full, clear, and exact description thereof, which will enable, others skilled in the art to which my. invention appertains to make and use the same. I V Hitherto the nicotin was. produced by extracting' tobacco by means of alcohol, distilling the extract thus obtained with water until the alcohol is evaporated, then adding caus tic lye, extracting the nicotin by shaking with ether, evaporating the latter, and drying the remainder over burnt chalk in a hydrogencurrent. Now this method is very circumstantial and not suited for producing nicotin and its salts on a larger scale. These disadvantages are obviated bymy new process, which is very simple and by means of which I am able to produce nicotin and its salts, especially salic'ylate of nicotin on a large scale and at comparatively low costs.

I proceed as follows: Tobacco or tobacco-.

waste are extracted with water, as hitherto, in

' order to produce-tobacco extract. This latter after'addition of an alkali is subjected to the distillation by means of steam. The distillate thus obtained is neutralized with a suitable tract containing sulfuric acid is-mixed with a in order to neutralize the acid extract.

lye of sodium hydra to of 1.3 specific weight a lye of carbonate or sodium of 18 Baum or of 1-. t specific weight is added, because the: nicotin better freed by means of carbonate of sodium than by swans of soda or sodium hydrate. The whole liquid is then distilled in a current of steam.

nicotin contained in the distillate with the sul- Theu To the distillate thus obtained sulfuric aci'i is added (twelve to thirteen kilogram parts of acid to one hundred kilograms of. tobacco extract) for the purpose of neutralizing the alkali and combining the furic acid, thus'producing sulfate of nicoti'n,

as otherwise by the concentration of the distillate the nicotin would evaporate with the steam. The quantity of sulfuric acid will have to bedistinctly determined for each process,

as the quantity of alkali used in the preceding part of the proces varies or depends upon the quan tity of the acid. The mixture is now evaporated until crystallization begins.

fate. The expression until crystallization begins is well understood by chemists. The heating or evaporation is' interrupted just when a thin skin of crystals is being, formed on the liquid. The formation of real crystals must be prevented. To the mixture is then added a lyeof caustic soda of 1.3 specific weight until the action is alkaline, whereby nicotin of the desiretipercentage is separated. The liquid is now dried by means of chlorid of calcium or water-free potash or other equivalent material in granular or powdered form and is separazed from the drying substance in any desirable manner-forexample. The nicotin 15 then by means of filtration. mxied with that quantity of salicylic acid as according to the formula is necessary for the formation of salicyl'ate of nicotin.

. Having thusdescribed my invention and inwhat manner thesame is to be performed, I

declare that what- I claim asmew, and desire to secure by Letters'Patent. is i The hercinbefore-descrihed process of ob taining nicotin consisting of mixing with tobacco extract containing sulfuric acid, a lye of sodium hydrate to neutralize the acid, dis: tilling the mixture. adding sulfuric acid to the distillate, evaporating until crystallization commences, and adding a lye of caustic soda to secure an alkaline reaction.-

In witness whereof I have hereunto set my hand in presence of two witnesses.

ALFRED KOELLI'KER. \Vitne scs: w

\V r 1.1mm! KCPPER, v GUSTAV Ensure.

"The

crystals are for the greater part sodium sul- 

